Abstract In this work, we report the synthesis of YbxZn1-xO nanoparticles (0.000 ≤x≤ 0.100) by polymer precursor method and the study of their vibrational and structural properties. Thermal analysis of the polymeric precursor showed that the thermal decomposition occurs in few stages, with the crystallization of the wurtzite structure taking place at a temperature below 500 C. Fourier transform infrared spectroscopy indicated the presence of Zn-O and Yb-O bonds. X-ray diffraction data showed the formation of the ZnO wurtzite phase for all samples. The application of the Rietveld method revealed a decrease in the average particle size and an increasing trend in unit cell volume as the Yb3+ content increased. Additionally, the nearest-neighbor bond lengths along and off the c-direction, as well as the bond angles, were calculated. The results obtained provided additional evidence on the efficiency of Yb3+ doping by the polymer precursor method.